浸渍-煅烧法合成纳米氧化铜的研究

纳米氧化铜是一种重要的功能材料,在高温超导、有机催化、传感器、锂离子电极材料等方面均具有广泛的应用前景.由于CuO在应用效果上与其形貌、粒径大小以及粒径分布有密切关系,因此,纳米CuO的可控研究仍具有重要意义.     

新铌酸盐晶体Na_（2．1）Ba_（0．9）Cu_（0．2）Nb_（4．8）O_

新铌酸盐晶体Ｎａ_（２．１）Ｂａ_（０．９）Ｃｕ_（０．２）Ｎｂ_（４．８）Ｏ_（１４．２）的合成张高科，欧阳世翕，吴伯麟（武汉工业大学非金属研究所新材料研究所，武汉４３００７０）许多铌酸盐晶体由于其优良的物理特性，常被作为功能材料广泛进行研究和应用［１?..     

苝环结构修饰的丙烯酰胺聚合物的合成及性质

近年来，红基元结构作为功能材料引起人们的广泛注意［１，２］，我们选择部分红颜料研究了其用于静电复印的光电性能取得了较好的结果［３～６］．但其难溶性阻碍了对它的进一步研究和应用，为此力图合成了红染料修饰的丙烯酰胺聚合物，该化合物溶解性、成膜性、加工性...     

多硫1，2-二硫醇烯配合物的研究进展

综述了近年来在新型多硫１，２－二硫醇烯配合物的合成、结构和性质方面的研究进展以及这些配合物作为分子导体、超导体、磁性材料和光电功能材料的应用前景。     

低温红外光谱研究CuO/γ-Al_2O_3上CO和NO选择性吸附

CuO作为催化剂的主要活性组分已应用于氧化、加氢、CO和碳氢化合物的燃烧,N0x还原等多种催化反应中,有关N0、CO在CuO上吸附的红外光谱研究已有一些报导.London和Bell曾研究CO和NO在CuO/SiO_2上的反应,他们根据红外光谱和动力学测量结果推测NO主要离解吸附于Cu~0上,而CO则吸附在Cu~+或Cu~(2+)上.Busca在未还原的CuO样品上,观测到CO在Cu~+上的红外吸收峰最强,从而认为体相为CuO的样品,铜在其表面主要由Cu~+并伴以Cu~(2+)构成.本文研究了CuO/γ-Al_2O_3上NO、CO单独、交替和共吸附时的低温红外光谱,证明当NO和CO共存时,NO选择吸附于Cu~(2+)上,而CO选择吸附于Cu~+上。     

介孔Ce1-xZrxO2负载的Cu基催化剂在富氢条件下催化CO选择性氧化

采用多元醇为模板剂合成了介孔Ce1-xZrxO2(x=0.2,0.35,0.5)固溶体材料,并以其为载体负载CuO制备了Cu基催化剂.应用透射电子显微镜、X射线衍射、程序升温还原、程序升温脱附和N2吸附-脱附等技术对载体及催化剂进行了表征,并研究了Zr的取代比例x值对载体和Cu基催化剂性能的影响.结果表明,所有Ce1-xZrxO2样品均为介孔材料,其中Ce0.5-Zr0.5O2载体样品有较大的比表面积(181m2/g),CuO/Ce0.5Zr0.5O2催化剂样品在富氢条件下有较高的催化CO选择性氧化反应的活性和选择性.与其他催化剂样品相比,CuO/Ce0.5Zr0.5O2催化剂样品中形成的活性中心更多,分散性更好,对CO的吸附量更大,CO脱附温度更低,活性组分与载体的相互作用更强。     

纳米SnO2微粉的制备与性能

纳米ＳｎＯ_２微粉的制备与性能刘杏芹，陶善文，沈瑜生（中国科学技术大学材料科学与工程系合肥２３００２６）关键词纳米微粉，二氧化锡，溶胶－凝胶法，气敏性能ＳｎＯ２作为一种功能基体材料，在气敏、湿敏、光学技术等方面已有广泛的应用，而ＳｎＯ２微粉或超微粉的?..     

CO和NO在CuO及Cu2O(110)表面吸附选择规律研究

采用离散变分Xα方法分别计算了CO和NO以C（或N）端顶位吸附在CuO（110）及Cu2O（110）表面上的基态势能曲线,结果表明：CO在Cu2O表面上的吸附强,而在CuO表面上的吸附弱;NO则在CuO表面上吸附强,在Cu2O表面上吸附弱．它们的吸附能的大小顺序为：CuO－NO＞Cu2O－CO＞Cu2O－NO＞CuO－CO．对于CuO－NO（或CO）吸附体系,主要是Cu的3d轨道与吸附分子的2π轨道间的相互作用;对于Cu2O－CO（或NO）吸附体系,则主要是吸附质分子的5σ及2π分子轨道与其顶位Cu1的4s及4p轨道和侧位Cu2的3d轨道相互作用．本文通过吸附势能曲线、态密度分析、成键分析及电荷转移量和方向等方面对实验现象做了合理的解释．     

CuO/Ce-Zr-La-O催化剂的表征及CO氧化活性

采用柠檬酸溶胶-凝胶法制备的Ce-Zr-La-O固溶体为载体，制备CuO／Ce-Zr-La-O催化剂，用XRD，Raman，TPR等实验技术对Ce-Zr-La-O固溶体及CuO／Ce-Zr-La-O的物相、Redox性能进行了表征。实验结果表明，Ce0.7Cr0.3-yLayO固溶体的还原性能与La含量有关，适量的La能促进固溶体的氧化还原。CuO的负载量为6％时，CuO／Ce0．7Zr0.15La0.15O的活性最高，高分散且与载体相互作用的CuO是CO氧化活性相。     

聚酯酸酐的合成与表征

聚酸酐具有优良的表面溶蚀性能，作为药物控释体系材料得到广泛的应用．以对（２ 羟基 乙氧基）苯甲酸和对（２ 甲基 ２羟基 乙氧基）苯甲酸分别与丁二酸酐，顺丁烯二酸酐和丁二酰氯反应得到六个含有酯基的新型二元酸单体，经熔融聚合得到聚酯酸酐．单体和聚合物经ＩＲ，１Ｈ ＮＭＲ和元素分析等表征．研究了催化剂对聚合物结构的影响．     

Microstructure and Photocatalytic Property of SiO<Subscript>2</Subscript>-TiO<Subscript>2</Subscript> Under Various Process Condition

Nanophase silica-titania particles were prepared by two different synthetic routes, namely, sol–gel and hydrothermal processing. The crystallinity and crystallographic phases, particle size and surface area of the materials were controlled by varying the calcination temperature, and/or the ratio of Si to Ti. It was determined by XRD that the crystallite sizes of SiO₂-TiO₂ prepared by sol–gel and hydrothermal processing decreased from 11 to 6 nm and 12 to 9 nm, respectively, as the mole fraction of silica was increased from 0.1 to 0.4. It is proposed that the presence of the amorphous silica suppresses the growth of anatase TiO₂ grains and their phase transformation to rutile. The photocatalytic decomposition rate of 1,4-dichlorobenzene (DCB) in aqueous solution with the sol–gel derived SiO₂-TiO₂ powder prepared at 750 °C was about 10 ± 5% higher than that observed with Degussa P25, whereas the SiO₂-TiO₂ samples prepared by hydrothermal processing at 250 °C showed a slightly lower decomposition rate than P25.     

Effects of gamma-irradiation on physicochemical state of surface and catalytic properties of CuO/MgO and NiO/MgO systems

Copper and nickel oxide samples supported on MgO were prepared by wet impregnation method. The obtained solids were heated at 350 °C and 450 °C. The extent of copper and nickel oxides was fixed at 16.7 mol%. The effect of g-irradiation (0.2-1.6 MGy) on the surface and catalytic properties of the solids were investigated. The techniques employed were XRD, nitrogen adsorption at -196 °C and H₂O₂ decomposition. The results revealed that the g-irradiation up to 0.8 MGy of CuO/MgO-450 °C effected a measurable decrease in the crystallite size of CuO phase with subsequent increase in its degree of ordering. Irradiation at a dose of 1.6 MGy brought about a complete conversion of MgO into Mg(OH)₂ during its cooling from 450 °C to room temperature via interacting with atmospheric water vapor. The S _BET and total pore volume of CuO/MgO precalcined at 350 °C and 450 °C increased progressively as a function of g-ray dose reached a maximum limit at 0.8 MGy. Gamma-irradiation of NiO/MgO-450 °C solids up to 0.8 MGy increased the degree of ordering of MgO and NiO phases without changing their crystallite size. The exposure of these solids to 1.6 MGy led to an effective transformation of some of NiO (not dissolved in MgO lattice) into Ni(OH)₂ via interacting with atmospheric water vapor during cooling from 450 °C to room temperature. Gamma-irradiation led to a measurable increase in the S _BET and V _p of NiO/MgO system. Gamma-irradiation of the two investigated systems resulted in both increase and decrease in their catalytic activities in H₂O₂ decomposition depending mainly on the irradiation dose and calcination temperature. This treatment, however, did not modify the mechanism of the catalytic reaction, but changed the catalytic active sites without changing their energetic nature. This revised version was published online in July 2006 with corrections to the Cover Date.     

Surfactant-free thermal decomposition route to phase pure tricobalt tetraoxide nanoparticles from cobalt(II)-tartrate complex

Tricobalt tetraoxide nanoparticles have been successfully synthesized following a ‘bottom-up’ approach by surfactant-free thermal decomposition of cobalt(II)-tartrate complex obtained by a modified sol–gel route. The synthesized complex was characterized by Fourier transform infrared (FT-IR) spectroscopy, elemental and thermogravimetric-differential thermal analysis (TG–DTA). The nanoparticles were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and Raman studies. The powder XRD pattern furnished evidence for a face-centered cubic structure of Co₃O₄. With the rise in calcination temperature from 400 through 500 to 600 °C, the average crystallite sizes of Co₃O₄ were found to increase from 28 through 36 to 46 nm. The TEM image revealed a faceted morphology of the as-synthesized Co₃O₄ nanoparticles. The high-resolution TEM image indicated the interplanar separation to be 0.28 nm which corresponds to the (220) plane in face-centered cubic Co₃O₄. The electron diffraction (ED) pattern showed single-crystalline nature of the synthesized nanoparticles. Raman spectrum showed four characteristic peaks of Co₃O₄ which further confirmed the phasic purity of the material.     

Synthesis of nanosized TiO2/SiO2 particles using microwave processes and their photocatalytic activity on the decomposition of orange II

The nanosized titania and TiO₂/SiO₂ particles were prepared by the microwave-hydrothermal method. The effect of physical properties TTIP/TEOS ratio and calcination temperature has been investigated. The major phase of the pure TiO₂ particle is of the anatase structure, and a rutile peak was observed above 800°C. In TiO₂/SiO₂ particles, however, no significant rutile phase was observed, although the calcination temperature was 900°C. No peaks for the silica crystal phase were observed at either silica/titania ratio. The crystallite size of TiO₂/SiO₂ particles decreases as compared to pure TiO₂ at high calcination temperatures. The TiO₂/SiO₂ particles show higher activity on the photocatalytic decomposition of orange II as compared to pure TiO₂ particles.     

Characterization of the calcination process of yttria

A complete characterization of the calcination of precipitates obtained from a continuous operation was carried out in this study. The precipitate was obtained by reacting yttrium nitrate and ammonia solutions in a MSMPR reactor. It precipitated out as yttrium hydroxide nitrate hydrate, which has the general form Y₂(OH)_6-x(NO₃)_x·y H₂O. This compound decomposed in consecutive steps with the last reaction occurring at 525°C.The calcination process was characterized by chemical analysis, X-ray diffraction analysis, DTA and TG. In addition, the physical characteristics of calcined powders, such as specific surface area, particle size distribution, pore volume distribution, X-ray crystallite size and conversion were measured as a function of calcination temperature and time. Finally, the kinetics of the reduction of surface area, the growth of crystallite size and conversion were also examined.     

Construction of 3D hierarchical SnO2 microspheres from porous nanosheets towards NO decomposition

Three-dimensional (3D) hierarchical architectures are currently attracting worldwide interest owing to their fascinating morphology-dependent properties and potential applications. Herein we constructed SnO₂ microspheres with 3D hierarchical flower-like architectures self-assembled with porous SnS₂ nanosheets by a facile hydrothermal method with subsequent calcination. The chemical and physical properties as well as photocatalytic application of SnO₂ microspheres were investigated. The size and morphology were examined with scanning electron microscopy and transmission electron microscopy. The phase and crystalline structure were determined with powder X-ray diffraction. The UV–Vis absorption property was determined with UV–Vis diffuse reflectance. The photocatalytic activities were evaluated with nitrogen monoxide (NO) decomposition under UV–Vis light irradiation. The effects of calcination temperature on morphology and NO decomposition were also studied.     

纯相和镍取代的Co_3O_4尖晶石催化剂用于N_2O直接分解(英文)

A series of NixCo1-xCo2O4(0 ≤ x ≤ 1) spinel catalysts were prepared by the co-precipitation method and used for direct N2O decomposition. The decomposition pathway of the parent precipitates was characterized by thermal analysis. The catalysts were calcined at 500 °C for 3 h and characterized by powder X-ray diffraction, Fourier transform infrared, and N2 adsorption-desorption. Nickel cobaltite spinel was formed in the solid state reaction between NiO and Co3O4. The N2O decomposition measurement revealed significant increase in the activity of Co3O4 spinel oxide catalyst with the partial replacement of Co2+ by Ni2+. The activity of this series of catalysts was controlled by the degree of Co2+ substitution by Ni2+, spinel crystallite size, catalyst surface area, presence of residual K+, and calcination temperature.     

Study of CuO/Ce0.8Zr0.2O2 catalysts for low-temperature CO oxidation

Summary Copper oxide catalysts supported on Ce_0.8Zr_0.2O₂ were prepared via an impregnation method and characterized by XRD and H₂-TPR techniques. The catalytic activity of the samples for low-temperature CO oxidation was investigated by means of a microreactor-GC system. The influence of calcination temperature, calcination time and different CuO content on the catalytic activity was studied. TPR analysis indicated that well-dispersed CuO was responsible for the low-temperature CO oxidation. The results of the investigation showed that the calcination temperature and CuO loadings had larger influence than the calcination time.     

Structural and optical characterization of Ag-doped TiO2 nanoparticles prepared by a sol–gel method

Undoped and silver-doped TiO₂ nanoparticles (Ti_1?x Ag _x O₂, where x?=?0.00?C0.10) were synthesized by a sol?Cgel method. The synthesized products were characterized by X-ray diffraction (XRD), particle size analyzer (PSA), scanning electron microscope (SEM), and UV?CVisible spectrophotometer. XRD pattern confirmed the tetragonal structure of synthesized samples. Average crystallite size of synthesized nanoparticles was determined from X-ray line broadening using the Debye?CScherrer formula. The crystallite size was varied from 8 to 33?nm as the calcination temperature was increased from 300 to 800?°C. The incorporation of 3 to 5% Ag⁺ in place of Ti⁴⁺ provoked a decrease in the size of nanocrystals as compared to undoped TiO₂. The SEM micrographs revealed the agglomerated spherical-like morphology of particles. SEM, PSA, and XRD measurements show that the particles size of the powder is in nanoscale. Optical absorption measurements indicated a red shift in the absorption band edge upon silver doping. Direct allowed band gap of undoped and Ag-doped TiO₂ nanoparticles measured by UV?CVis spectrometer were 3.00 and 2.80?eV, respectively, at 500?°C.     

Studies of the surface wettability and hydrothermal stability of methyl-modified silica films by FT-IR and Raman spectra

Fourier transform infrared (FT-IR) and Raman spectroscopy were employed to study the hydrothermal stability and the influence of surface functional groups on the surface wettability of methyl-modified silica films. The surface free energy parameters of the silica films were determined using the Lifshitz-van der Waals/acid–base approach. The thermal decomposition mechanisms of the CH₃ groups in the methyl-modified silica material are proposed. The results show that with the increase of methyltriethoxysilane (MTES)/tetraethylorthosilicate (TEOS) ratio, the surface free energy and surface wettability of the silica films decrease greatly. This is mainly because of the contribution of the acid–base term; the intensity of Si–CH₃ groups increases at the expense of the intensity of O–H groups in the samples. The surfaces of the methyl-modified silica films exhibited predominantly monopolar electron-donicity. The contact angle on the silica film surface reaches its maximum value when calcination is performed at 350 °C. Thermogravimetric analysis implies that some low molecular weight species, such as H₂, CH₄, and C, are eliminated upon thermal decomposition of the –CH₃ groups. The Si–CH₃ and –CH₃ vibrational bands diminish in intensity as the calcination temperature is increased, disappearing completely when the calcination temperature is increased to 600 °C. When the calcination temperature is increased to 750 °C, the free carbon and CSi₄ species will be formed.